Simultaneous Determination of 5 Components in the Classical Formula Huaihua San by HPLC Wavelength Switching Method / 中国药房

OBJECTIVE：To develop a method for simultaneous determination of 5 components in classical formula Huaihua san，including rutin ，naringin，neohesperidin，quercetin and pulegone. METHODS ：HPLC wavelength switching method was adopted. The determination was performed on Cosmosil C 18 column with mobile phase consisted of acetonitrile- 0.05％ phosphoric acid solution （gradient elution ）at the flow rate of 1.0 mL/min. The detection wavelengths were set at 257 nm for rutin ，283 nm for naringin and neohesperidin ，254 nm for quercetin ，252 nm for pulegone ，respectively. The column temperature was set at 30 ℃， and sample size was 10 μL. RESULTS：The linear range was 21.7-2 170 μg/mL for rutin，46-4 600 μg/mL for naringin，22.3- 2 230 μg/mL for neohesperidin，0.96-96 μg/mL for quercetin，2.7-270 μg/mL for pulegone（all r＞0.999），respectively. RSDs of precision，stability（24 h）and reproducibility tests were all lower than 2％（n＝6）. Average recoveries were 100.70％，99.31％， 101.10％，100.03％ and 99.63％（all RSD ＜2％，n＝9）. Among 3 batches of Huaihua san samples ，the contents of above 5 components were 20.055-22.615，25.557-27.806，11.428-13.250，0.350-0.478，2.372-4.011 mg/g，respectively. CONCLUSIONS ： Established method is simple ，accurate and reproducible ，and could be used for the simultaneous determination of 5 components in Huaihua san.

Simultaneous Determination of 12 Components in the Classical Formula Sanhua Tang by HPLC-multi-wavelength Switching Technology / 中国药房

OBJECTIVE：To establish a method for simultaneous determination of 12 components including naringin ， hesperidin，neohesperidin，aloe emodin ，rhein，notopterol，emodin，honokiol，isoimperatorin，magnolol，chrysophanol and physcion in classical formula Sanhua tang. METHODS ： HPLC-multi-wavelength switching technology was adopted. The determination was performed on COSMOSIL C 18 with mobile phase consisted of acetonitrile- 0.1％ phosphoric acid （gradient elution）at the flow rate of 1.0 mL/min. The detection wavelength was 280 nm（naringin，hesperidin，neohesperidin），254 nm （aloe emodin ，rhein，chrysophanol，emodin methyl ether ），310 nm（notopterol，emodin，honokiol，isoimperatorin，magnolol）. The column temperature was set at 30 ℃，and the sample size was 10 μL. RESULTS：A total of 12 components were well separated without negative interference. The linear range of naringin ，hesperidin，neohesperidin，aloe emodin ，rhein，notopterol， emodin，honokiol，isoimperatorin，magnolol，chrysophanol and physcion were 55.4-5 540，3.8-380，45.6-4 560，1.2-120， 2.1-210，2.2-220，2-200，2.4-240，0.8-80，1.2-120，1.7-170，1.1-110 μg/mL（R 2≥0.999 6），respectively. The detection limits were 0.064，0.024，0.053，0.018，0.020，0.041，0.050，0.091，0.030，0.180，0.028 and 0.083 μg/mL，respectively. The limits of quantitation were 0.213，0.075，0.174，0.060，0.063，0.138， 0.166，0.323，0.130，0.600，0.094 and 0.275 μ g/mL，respec- 9721004） tively. RSDs of precision ，stability （24 h） and repeatability 2633531778@qq.com tests were all lower than 2％（n＝6）. Average recoveries were 99.54％，99.69％，100.01％，99.93％，100.36％，99.65％， 100.03％，100.47％，99.97％，100.68％，99.90％，100.17％ （all RSDs were lower than 2％，n＝6），respectively. CONCLUSIONS ：Established HPLC-multi- wavelength switching technology is simple ，specific and stable ，which could be used for the simultaneous determination of 12 components in Sanhua tang as naringin，hesperidin，neohesperidin.

Simultaneous Determination of Eight Active Components in Material Benchmark of Shentong Zhuyutang by HPLC-DAD Wavelength Switching / 中国实验方剂学杂志

Objective::To develop high performance liquid chromatography-diode array detector (HPLC-DAD) wavelength switching for simultaneously determining the contents of inosine, loganic acid, chlorogenic acid, amygdalin, hydroxysafflor yellow A, gentiopicroside, ferulic acid and liquiritin in 15 batches of material benchmarks of Shentong Zhuyutang. Method::The quantitative analysis was carried out on a Thermo Hypersil GOLD C18 column (4.6 mm×250 mm, 5 μm) with mobile phase of acetonitrile-0.1%phosphoric acid aqueous solution for gradient elution, the flow rate was 1.0 mL·min-1, the detection wavelengths were set as 248 nm (0-11 min, inosine), 235 nm (11-14 min, loganic acid), 324 nm (14-16 min, chlorogenic acid), 220 nm (16-19 min, amygdalin and hydroxysafflor yellow A), 274 nm (19-26 min, gentiopicroside), 247 nm (26-54 min, ferulic acid and liquiritin), the column temperature was maintained at 25 ℃. According to the contents of eight active components in 15 batches of material benchmarks, orthogonal partial least squares discriminant analysis (OPLS-DA) in SIMCA 14.1 was used to evaluate the quality difference of each batch of samples. Result::Each component had good separations, the linear ranges of the above 8 components were 2.1-67.2, 1.812 5-58, 1.937 5-62, 5.212 5-166.8, 8.45-270.4, 7.075-226.4, 1.775-56.8, 3.875-124 mg·L-1, respectively (r≥0.999 6). The average recoveries of them were 99.23%, 100.09%, 99.33%, 98.85%, 99.15%, 98.75%, 99.42%, 98.96%, respectively (RSD<2%). The contents of the above eight components in 15 batches of material benchmarks were 0.183 5-0.250 3, 0.173 1-0.265 3, 0.069 5-0.169 8, 0.959 2-1.458 2, 1.905 4-2.553 3, 0.933 3-1.997 5, 0.084 6-0.143 4, 0.212 5-0.704 3 mg·g-1, respectively. Liquiritin, ferulic acid, gentiopicroside and hydroxysafflor yellow A were determined to have significant impact on the quality of different batches of material benchmarks of Shentong Zhuyutang through OPLS-DA. Conclusion::The established method for simultaneous determination of multi-components is reliable, simple and in line with the requirements of methodological verification. It is suitable for the quality control of research and development of compound preparations of Shentong Zhuyutang.

Quality evaluation of Styrax based on quantitative determination of 7 chemical components using HPLC wavelength switching method and chemometrics / 中国中药杂志

In order to evaluate the quality of Styrax more comprehensively,this study attempted to establish an HPLC wavelength switching method to simultaneously determine the content of seven compounds in Styrax,and chemometrics were used to analyze the quality difference between different sources of Styrax,and finally establish a characteristic chromatogram of Styrax. The column was Agilent ZORBAX Extend C18( 4. 6 mm×250 mm,5 μm) with phase a mixture of acetonitrile-0. 1% phosphoric acid aqueous solution as the mobile phase in a gradient elution procedure; the detection wavelength was set as follows: 0-13. 5 min,194 nm( benzoic acid);13. 5-20. 5 min,278 nm( cinnamic acid); 20. 5-32 min,194 nm( benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid); 32-55 min,241 nm( abietic acid). The methodological verification results showed that when the injection masses of benzoic acid,cinnamic acid,benzyl benzoate,benzyl cinnamate,cinnamyl cinnamate,dehydroabietic acid and abietic acid were0. 006 948-0. 694 8,0. 001 426-0. 142 6,0. 013 16-0. 658 0,0. 006 148-0. 614 8,0. 008 035-0. 803 5,0. 002 121-0. 212 1,and0. 010 172-1. 017 2 μg,respectively,there were good linear relationship between injection mass and peak area. The average recovery rates of seven compounds were in the range from 94. 34% to 105. 8%,and all RSD were less than 3. 0%( n = 6). The methodological verification results showed that the developed HPLC wavelength switching method has good accuracy and repeatability. The results of the sample analysis showed that the quality of Styrax from different sources was quite different. The chromatogram of Styrax reference material( S1) was used as the reference chromatogram to calculate the fingerprint similarity of each batch of samples. The results showed that the similarities of samples S2-S10 were 0. 952,0. 949,0. 981,0. 351,0. 751,0. 969,0. 979,0. 992 and 0. 971,respectively.The similarity values of other batches samples were satisfactory,except for sample S5 and S6,indicating that the quality difference among these samples is small. The similarity values of S11-S20 were 0. 060,0. 055,0. 054,0. 285,0. 092,0. 002,0. 044,0. 044,0. 044,and 0. 040,respectively. The results showed that compared with the sample S1,there was a large quality difference among S11-S20. Based on the chromatograms of S1-S10,the HPLC characteristic chromatograms of Styrax was established and the purpose is to give reference to other pharmaceutical researchers. The newly developed HPLC wavelength switching method have the advantages of simplicity,reproducibility and specificity,and the developed HPLC characteristic chromatograms provided a reference method for the overall quality evaluation of Styrax.

Simultaneous Determination of 7 Components in Niuhuang Qingwei Pills by HPLC-wavelength Switching Method / 中国药房

OBJECTIVE： To develop a method for simultaneous determination of 7 components of Niuhuang qingwei pills as chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol. METHODS： HPLC-wavelength switching method was adopted. The determination was performed on Agilent ZORBAX SB-C18 column with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid （B） gradient elution at the flow rate of 1.0 mL/min. The detection wavelengths were set at 348 nm （chlorogenic acid）， 238 nm （geniposide）， 330 nm （forsythoside A）， 280 nm （narirutin and baicalin）， 237 nm （ammonium glycyrrhetate）， 254 nm （chrysophanol）. The column temperature was 30 ℃， and sample size was 10 μL. RESULTS： The linear ranges of chlorogenic acid， geniposide， forsythoside A， narirutin， baicalin， ammonium glycyrrhetate， chrysophanol were 0.011 67-0.233 4 μg （r＝0.999 4）， 0.042 91-0.858 1 μg （r＝0.999 4）， 0.125 0-2.500 μg （r＝0.999 9）， 0.118 0- 2.360 μg （r＝0.999 9）， 0.119 6-2.392 μg （r＝0.999 7）， 0.030 57-0.611 4 μg （r＝0.999 6）， 0.006 201-0.124 0 μg（r＝0.999 4）， respectively； the limits of quantitation were 1.167， 0.858， 1.250， 1.180， 1.196， 0.611， 0.620 μg/mL， respectively； RSDs of precision tests were 0.98％， 1.04％， 0.59％， 1.50％， 0.83％， 1.24％ and 1.32％ （n＝6）， respectively. RSDs of stability tests were 1.21％， 0.97％， 1.42％， 0.71％， 0.98％， 1.87％ and 1.63％ （n＝6， 12 h）， respectively. Average recoveries were 98.32％， 98.11％， 98.81％， 98.50％， 98.30％， 98.16％ and 97.83％， and the RSDs were 1.37％， 1.41％， 0.64％， 1.01％， 1.18％， 1.16％ and 1.16％ （n＝6）， respectively. CONCLUSIONS： Established method is easy and reproducible. It can be used for the quality control of Niuhuang qingwei pills.

Simultaneous Determination of Dehydrocorydine and Salvianolic Acid B in Shuangshen Tongguan Capsules by HPLC-dual Wavelength Switching Method / 中国药房

OBJECTIVE： To develop an method for determining the contents of dehydrocorydine and salvianolic acid B in Shuangshen tongguan capsules simultaneously. METHODS： The HPLC-dual wavelength switching method was used. The determination was performed on Waters symmetry C18 column with mobile phase consisted of acetonitrile-0.05％ phosphoric acid solution （gradient elution） at the flow rate of 1.0 mL/min， the detection wavelength was 286 nm （salvianolic acid B） and 336 nm （dehydrocorydine）. The column temperature was maintained at 25 ℃， and sample size was 10 μL. RESULTS： Under this condition， dehydrocorydaline and salvianolic acid B could be separated in baseline. The linear range of them were 0.157-1.259 μg and 0.391-3.131 μg （r＝0.999 9）. RSDs of precision， reproducibility and stability tests （within 24 h） were all lower than 2.00％ （n＝6-10）. The average recovery rates were 101.61％ and 102.85％ （RSD＝3.59％ and 2.85％， n＝6）. CONCLUSIONS： Established HPLC-dual wavelength switching method can be used for simultaneous determination of dehydrocorydine and salvianolic acid B in Shuangshen tongguan capsules. The method is simple and rapid， and can be used for the quality control of Shuangshen tongguan capsule.

Hplc fingerprint and chemical pattern recognition of valeriana jatamansi / 中国药学杂志

OBJECTIVE: To establish the HPLC fingerprint of Valeriana jatamansi and provide a reference for its effective quality control. METHODS: The HPLC-DAD analysis was performed on Diamonsil C18 column (4.6 mm×250 mm, 5 μm), with acetonitrile (A)-0.1% formic acid (B) solution as the mobile phase for gradient elution, the detection wavelength was set at 327 nm (0-33 min) and 256 nm (33-90 min), the flow rate was 1.0 mL•min-1, and the column temperature was maintained at 30 ℃. The fingerprints of 25 batches of Valeriana jatamansi samples were analyzed by similarity analysis, hierarchical clustering analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares discriminant analysis (PLS-DA). RESULTS: The fingerprints of 25 batches of Valeriana jatamansi samples were established. There were 36 common peaks in the fingerprints and nine common peaks were identified by reference substances. The fingerprints similarity of 18 batches of samples was over 0.9, and the samples were classified into two groups. Six components were the main markers that cause differences in different batches of samples, including valepotriate, acevaltrate, isochlorogenic acid A, and some others. CONCLUSION: HPLC fingerprint combined with recognition of chemical pattern can reflect the intrinsic quality of Valeriana jatamansi, which may provide reference for the quality control and evaluation of Valeriana jatamansi.

Multi-component Quantification Analysis and Overall Quality Evaluation of Dieda Pills / 中国药学杂志

OBJECTIVE: To establish an HPLC method for simultaneous determination of nine components, i.e., paeoniflorin, naringin, hesperidin, neohesperidin, paeonol, asperosaponin , glycyrrhizic acid, curcumin and acetyl-11-keto-beta-boswellic acid, and evaluate the overall quality of Dieda pills. METHODS: The analysis was performed on an Agilent 1260 Infinity LC System with a diode array detector. The chromatographic separation was performed on Agilent Poroshell 120 EC-C18 (4.6 mm×100 mm, 2.7 μm) column. The mobile phase was a mixture of acetonitrile (mobile phase A) and water containing 0.1% phosphoric acid aqueous solution (mobile phase B). The gradient elution program was as follows: 5%-18%A for 0-7 min, keeping 18%A for 7-15 min, 18%-35%A for 15-27 min, 35%-60%A for 27-32 min, 60%-95%A for 32-42 min, keeping 95%A for 42-45 min.The flow rate was set at 1.0 mL•min-1, the column temperature was maintained at 30 ℃ and the injection volume was 5 μL. The detection wavelength was set at 230 nm for paeoniflorin, 283 nm for naringin, hesperidin and neohesperidin, 274 nm for paeonol, 212 nm for asperosaponin , 251 nm for glycyrrhizic acid, 440 nm for curcumin and 251 nm for acetyl-11-keto-beta-boswellic acid, respectively. RESULTS: All the nine components achieved good separation.The linear ranges fell with in the range of 0.1-1.0 μg for paeoniflorin, naringin, neohesperidin andacetyl-11-keto-beta-boswellic acid, 0.2-2.0 μg for hesperidin and asperosaponin , 0.04-0.4 μg for paeonol, 0.02-0.2 μg for glycyrrhizic acid and 0.01-0.1 μg for curcumin,respectively(r2≥0.999 8). The average recoveries (n=6) were 96.95%-100.4% and the RSDs were 0.21%-0.81%. CONCLUSION: The developed method is simple, accurate, reliable, and can be used for the overall quality control and quality evaluation of Dieda pills.

Simultaneous determination of seven constituents in Compound Yi’anning Pills by HPLC coupled with wavelength switching method / 中草药

Objective: To establish an HPLC method for the simultaneous content determination of seven constituents in Compound Yi’anning Pills (CYP). Methods: The determination was performed on Shim-pack GIST C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid (gradient elution: 0-5 min, 5% acetonitrile; 5-12 min, 5%-12% acetonitrile; 12-17 min, 12%-20% acetonitrile; 17-30 min, 20% acetonitrile; 30-36 min, 20%-50% acetonitrile; 36-45 min, 50%-80% acetonitrile; 45-70 min, 80% acetonitrile) at the flow rate of 1.0 mL/min. The detection wavelength was set at 203 nm for notoginsenoside R1, ginsenoside Rg1, and ginsenoside Rb1, 220 nm for schisantherrin A, 250 nm for schisandrin, 268 nm for salvianolic acid B, and 270 nm for tanshinone IIA. The column temperature was set at 35 ℃ and the injection volume was 10 μL. Results: The linear range of detection concentration was 0.015-0.150 mg/mL for notoginsenoside R1, 0.077-0.766 mg/mL for schisandrin, 0.006-0.062 mg/mL for salvianolic acid B, 0.009-0.092 mg/mL for buddleodide, 0.050-0.503 mg/mL for ginsenoside Rg1, 0.067-0.670 mg/mL for ginsenoside Rb1, and 0.011-0.108 mg/mL for tanshinone IIA. Average recoveries respectively were 99.5%, 99.8%, 99.2%, 98.9%, 96.9%, 98.8%, and 97.1%. Conclusion: The method is simple, effective, and accurate, which can be used for simultaneous determination of seven active constituents in CYP.

Simultaneous determination of nine ingredients in Shenkangling granules by HPLC wavelength switching method / 国际药学研究杂志

Objective: To establish an HPLC wavelength switching method for the simultaneous content determi- nation of verbascoside,paederosidic acid methyl ester,asperulosidic acid,asperuloside,calycosin7-O-β-D-glucopyran- oside,ononin,calycosin,formononetin and batatasinin Shenkangling granules(Radix Rehmanniae,Herba Hedyotis Diffusae,Radix Astragali,Rhizoma Dioscoreae,etc.). Methods: The Shenkangling granules were extracted with 50% aqueous methanol to prepare the test solution. The HPLC analysis was performed on thermostatic Agilent Eclipse XDB-C18 (250 mm×4.6 mm,5 μm)a 30℃,with the mobile phase consisting of acetonitrile-0.2% phosphoric acid solution at 0.9 ml/min flow rate in a gradient elution manner,and the detection wavelength was set at 334,238,254 and 270 nm, respectively. Results The above mentioned nine compounds showed good linearity in turn within the range of 3.09- 61.80,3.67-73.40,1.98-39.60,2.51-50.20,1.39-27.80,1.06-21.20,0.87-17.40,2.79-55.80,and 2.16-43.20 μg/ml, respectively,and their average recovery was 99.34%,100.03%,97.67%,98.63%,97.96%,96.93%,97.48%,99.87%, and 98.95% with the RSD of 0.88%,1.15%,1.28%,1.49%,0.99%,1.41%,1.37%,0.72%,and 1.25%,respectively.Conclusion: The method is easy to operate,repeatable,and can be used for quality control of Shenkangling granules.

Simultaneous Determination of Six Components in Ganyan Kangfu Pills by HPLC / 中国药师

Objective:To establish a wavelength switching HPLC with gradient elution for the simultaneous determination of six active components, [(R,S)-goitrin, salvianolic acid B, tanshinone IIA, luteolin-7-glucoside, 4-hydroxyacetophenone and scoparone ] in Ganyan Kangfu pills .Methods:An Agilent TC-C18 (250 mm ×4.6 mm, 5 μm) chromatographic column was used with the mobile phase consisting of acetonitrile and 0.1％ phosphoric acid solution with gradient elution .The flow rate was 0.9 ml· min-1 , and the column temperature was 25 ℃.( R,S)-Goitrin was detected at 245 nm, salvianolic acid B and tanshinone IIA were detected at 270 nm, luteolin-7-glucoside was detected at 348 nm, 4-hydroxyacetophenone and scoparone were detected at 278 nm.The sample volume was 10 μl.Results:The linear range of (R,S)-goitrin, salvianolic acid B, tanshinone ⅡA, luteolin-7-glucoside, 4-hydroxyacetophe-none and scoparone was 1.99-49.75 μg· ml-1(r=0.9999), 18.66-466.50 μg· ml-1(r=0.9994), 2.25-56.25 μg· ml-1(r=0.9998), 2.62-65.50 μg· ml-1(r=0.9998), 2.48-62.00 μg· ml-1(r=0.9992) and 2.55-63.75μg· ml-1(r=0.9996), respectively.The average recovery was 98.42％(RSD=0.83％), 99.56％(RSD=1.04％), 97.96％(RSD=1.53％), 96.84％(RSD=0.78％), 98.10％(RSD=1.44％) and 97.82％(RSD=1.34％)(n=6), respectively.Conclusion: The method with good reproducibility is simple and accurate , which provides a new way for the quality evaluation of Ganyan Kangfu pills .

Simultaneous determination of twelve constituents in nüjin pills by hplc combined with wavelength switching / 中国药学杂志

OBJECTIVE: To establish an HPLC method for simultaneous determination of 12 constituents in Nüjin pills. METHODS: The analysis was carried out on Agilent Eclipse plus C18 column(4.6 mm×250 mm,5 μm), using a mobile phase of acetonitrile (A)-0.2%formic acid solution (B) by a gradient elution program (0-25 min, 10%-35% A; 25-37 min, 35%-59% A; 37-40 min, 59%-75% A) at a flow rate of 1 mL•min-1 at 30 ℃. The detection wavelength was set at 230 nm in the first 20 min, and then changed to 270 nm between 20 and 40 min. RESULTS: The linear ranges of paeoniflorin, liquiritin, ferulicacid, narirutin, aurantiamarin, baicalin, wogonoside, cinnam aldehyde, baicalein, paeonol, ammonium glycyrrhetate and wogonin fell within the ranges of 0.011-1.062 μg, 0.002-0.237 μg, 0.003-0.259 μg, 0.006-0.641 μg, 0.029-2.925 μg, 0.033-3.339 μg, 0.008-0.834 μg, 0.003-0.258 μg, 0.008-0.772 μg, 0.008-0.824 μg, 0.007-0.724 μg and 0.005-0.539 μg, respectively. The recoveries were 99.3%, 98.4%, 99.1%, 99.4%, 99.5%, 99.6%, 99.4%, 99.2%, 99.0%, 99.6%, 99.1%, and 99.4%, respectively. The relative standard deviations were 0.35%, 1.02%, 0.33%, 0.38%, 0.18%, 0.27%, 0.40%, 0.74%, 0.53%, 0.16%, 0.08% and 0.21%, respectively (n=6). CONCLUSION: This method is simple, accurate and convenient for the quality control of Nüjin pills.

Simultaneous Determination of Five Components in Guilong Kechuanning Tablets by UPLC with Wave-length Switching / 中国药师

Objective:To develop a UPLC method for the simultaneous determination of 5 components in Guilong Kechuanning tablets including paeoniflorin, berberine hydrochloride, alkaloid, cinnamic acid and cinnamaldehyde. Methods:An ACQUITY UPLC BEH C18(2.1 mm ×100 mm,1.7 μm)chromatographic column was used;the mobile phase was acetonitrile(A)–0.1% formic acid solution (B) with gradient elution (0-10 min, 85% A;10-13 min, 10% A;13-15 min, 85% A) at a flow rate of 0. 4 ml·min-1, the detection wavelengths were:0-1. 8 min, 230 nm;1. 8-6. 0 min, 345 nm;6. 0-9. 0 min, 285 nm;9. 0-12. 0 min, 345 nm, and the column temperature was 30℃. Results:The linear range of paeoniflorin, berberine hydrochloride, alkaloid, cinnamic acid and cinna-maldehyde was 0. 060-1. 202 μg(r=0. 9999),0. 100-2. 010 μg(r=0. 9999),0. 040-0. 794 μg(r=0. 9994),0. 015-0. 302 μg(r=0.9999) and 0.042-0.850 μg(r =0.9999), the average recovery (n = 6) was 99.63%,99.26%,100.17%,98.80% and 100. 26%, and the RSDs were 0. 39%,0. 97%,0. 73%,1. 00% and 0. 71%, respectively. Conclusion:The method is simple, accu-rate and reproducible. It can be used for the quality control of Guilong Kechuanning tablets.

Simultaneous Determination of Five Components in Guilong Kechuanning Tablets by UPLC with Wave-length Switching / 中国药师

Objective:To develop a UPLC method for the simultaneous determination of 5 components in Guilong Kechuanning tablets including paeoniflorin, berberine hydrochloride, alkaloid, cinnamic acid and cinnamaldehyde. Methods:An ACQUITY UPLC BEH C18(2.1 mm ×100 mm,1.7 μm)chromatographic column was used;the mobile phase was acetonitrile(A)–0.1% formic acid solution (B) with gradient elution (0-10 min, 85% A;10-13 min, 10% A;13-15 min, 85% A) at a flow rate of 0. 4 ml·min-1, the detection wavelengths were:0-1. 8 min, 230 nm;1. 8-6. 0 min, 345 nm;6. 0-9. 0 min, 285 nm;9. 0-12. 0 min, 345 nm, and the column temperature was 30℃. Results:The linear range of paeoniflorin, berberine hydrochloride, alkaloid, cinnamic acid and cinna-maldehyde was 0. 060-1. 202 μg(r=0. 9999),0. 100-2. 010 μg(r=0. 9999),0. 040-0. 794 μg(r=0. 9994),0. 015-0. 302 μg(r=0.9999) and 0.042-0.850 μg(r =0.9999), the average recovery (n = 6) was 99.63%,99.26%,100.17%,98.80% and 100. 26%, and the RSDs were 0. 39%,0. 97%,0. 73%,1. 00% and 0. 71%, respectively. Conclusion:The method is simple, accu-rate and reproducible. It can be used for the quality control of Guilong Kechuanning tablets.

Rapid Quality Evaluation of Huoxiang Zhengqi Tincture (II): Simultaneous Determination of Seven Components in Huoxiang Zhengqi Tincture by UPLC with Wavelength Switching Detection / 中国药学杂志

OBJECTIVE: To investigate a rapid approach for quality evaluation of Huoxiang Zhengqi Tincture. METHODS: Hesperidin, glycyrrhizic acid, imperatorin, honokiol, isoimperatorin, magnolol and atractylodin in Huoxiang Zhengqi Tincture were determined by ultra performance liquid chromatography (UPLC) method combined with wavelength switching detection technology. The sample was injected directly without preprocessing. The separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm×100 mm, 1.8 μm) and the column temperature was maitained at 40℃. The mobile phase was composed of acetonitrile and 0.1% phosphoric acid with gradient elution at a flaw rate of 0.3 mL·min-1. Hesperidin was detected at 284 nm; glycyrrhizic acid was detected at 250 nm; imperatorin, honokiol, isoimperatorin and magnolol were detected at 300 nm; atractylodin was detected at 340 nm. RESULTS: The calibration curves of the seven components showed good linearity within their test ranges. The average recoveries for hesperidin, glycyrrhizic acid, imperatorin, honokiol, isoimperatorin, magnolol and atractylodin were 99.3%, 99.5%, 101.5%, 99.3%, 100.6%, 99.0% and 99.6%, respectively. And there were great variations among the contents of glycyrrhizic acid, imperatorin, isoimperatorin and atractylodin in 28 batches of samples from 13 manufactures. CONCLUSION: The proposed method is accurate, simple and rapid, thus providing basis for comprehensive quality control of Huoxiang Zhengqi Tincture.

Simultaneous Determination of 4 Components in Fufang Kushen Shuiyangsuan Powder by RP-Ion Pair HPLC with Wavelength Switching / 中国药师

Objective: To develop a RP-ion pair HPLC with wavelength switching for the simultaneous determination of 4 components (marine, oxymarine, salicylic acid, benzoic acid) in Fufang Kusheng Shuiyangsuan powder.Methods: An Agilent ZORBAX SB-C18 column(150 mm× 4.6 mm, 5 μm) was used;the mobile phase was acetonitrile (A)-0.1% phosphoric acid solution (0.2 g sodium heptanesulfonate was added to 100 ml solution) at a flow rate of 1.0 ml·min-1;the detection wavelength was 220 nm in 0-12 min and 280 nm in 12-25 min;the column temperature was 30℃.Results: The linear range of marine, oxymarine, salicylic acid and benzoic acid was 0.006 030-0.120 6 μg (r=0.999 4), 0.016 56-0.331 2 μg (r=0.999 9), 0.717 1-14.34 μg (r=0.999 9) and 0.512 0-10.24 μg (r=0.999 9), respectively;the average recovery was 98.14%, 97.20%, 97.05% and 98.39% with the RSDs of 1.38%, 0.32%, 0.81% and 1.26%(n=6) , respectively.Conclusion: The method is simple and rapid, and can be applied in the simultaneous determination of 4 components in Fufang Kusheng Shuiyangsuan powder.

Simultaneous Determination of 5 Components in Xiaoer Qingyan Granules by HPLC / 中国药房

OBJECTIVE:To develop a method for simultaneous determination of harpagide,harpagoside,chlorogenic acid, caffeic acid and phillyrin in Xiaoer qingyan granules. METHODS:HPLC method was adopted. The determination was performed on Zorbax SB-C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution (gradient elution) at a flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm (0-13 min,harpagide),327 nm (13-25 min,chlorogenic acid and caffeic acid),277 nm(25-29 min,phillyrin),210 nm(29-40 min,harpagosid);the column temperature was 30℃,and sam-ple size was 10 μL. RESULTS:The linear ranges of harpagide,harpagosid,chlorogenic acid,caffeic acid and phillyrin were 8.400-168.0 ng(r=0.9996),11.30-226.0 ng(r=0.9998),128.8-257.6 ng(r=0.9993),8.110-162.2 ng(r=0.9996),29.69-593.8 ng(r=0.9994),respectively. LOQs of the 5 components were 33.39,451.2,515.2,324.5,1188 ng/mL;LODs were 8.348, 112.8,128.8,81.12,297.0 ng/mL,respectively;RSDs of precision,stability and reproducibility tests were all lower than 2.0%. The recoveries were 96.39%-98.64%(RSD=0.83%,n=6),96.60%-98.89%(RSD=0.89%,n=6),96.28%-99.22%(RSD=1.25%,n=6),96.49%-99.54%(RSD=1.16%,n=6),96.26%-99.70%(RSD=1.30%,n=6),respectively. CONCLUSIONS:The method is simple,accurate and suitable for simultaneous determination of 5 components in Xiaoer qingyan granules

Simultaneous Determination of Chlorogenic Acid and Mangiferin in Yinhua Mangguo Tablets by Wave-length Switching HPLC / 中国药师

Objective:To establish a wavelength switching HPLC method for the simultaneous determination of chlorogenic acid and mangiferin in Yinhua Mangguo tablets. Methods:An Agilent ZORBAX Eclipse XDB-C18 (150 mm × 4. 6 mm, 5 μm) column was used. The mobile phase was methanol-water containing 0. 2% phosphoric acid with gradient elution at the flow rate of 1. 0 ml· min-1;the detection wavelength was 327 nm(0-8 min) for chlorogenic acid and 258 nm(8-20 min) for mangiferin. Results:Chlorogenic acid had good linearity within the range of 0. 140-2. 516 μg, and the average recovery was 99. 4% with RSD of 1. 2% (n=9). Mangiferin had good linearity within the range of 0. 042-0. 761 μg, and the average recovery was 99. 9% with RSD of 1. 4% (n=9). Conclu-sion:The method is simple, accurate and reproducible. It can be used to determine chlorogenic acid and mangiferin in Yinhua Mang-guo tablets with the same chromatogram conditions.

HPLC Wavelength Switching Simultaneous Determination for the Contents of Mangiferin and Hesperidin inYinhua Mangguo Tablets / 中国中医药信息杂志

Objective To establish an HPLC method of wavelength switching simultaneous determination for the contents of mangiferin and hesperidin inYinhua Mangguo Tablets.Methods Agilent ZORBAX Eclipse XDB-C18 (4.6 mm×150 mm, 5 μm) column was used. The mobile phase was methanol-water containing 0.2% phosphoric acid with gradient elution mode at the flow rate of 1.0 mL/min; the detection wavelength was 258 nm (0–20 min) for mangiferin, 283 nm (20–50 min) for hesperidin.Results Mangiferin had a good linearity in the range of 0.042–0.761 μg, and the average recovery was 99.86%, with RSD of 1.5% (n=9). Hesperidin had a good linearity in the range of 0.076–1.361 μg, and the average recovery was 99.91%, with RSD of 0.7% (n=9).Conclusion The method is simple, accurate and reproducible, which can be used to the quality control ofYinhua Mangguo Tablets.

Simultaneous determination of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in xixian fengshi wan by joint wavelength switching HPLC gradient elution method / 第二军医大学学报

Objective To establish a joint wavelength switching HPLC gradient elution method for simultaneous determination of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wan. Methods A Kromasil C18 column (4. 6 mm × 250 mm, 5 μm) was used with a mobile phase A; acetonitrile-methano (2: 1) and mobile phase B: 0. 05% acetic acid solution with gradient elution. The flow rate was 1. 0 mL/min; the injection volume was 20 μL; darutoside, kirenol and darutigenol were detected at 215 nm, and fangchinoline and d-tetrandrine were detected at 280 nm. Results In the given concentration range, the linearity ranges of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine were 6. 45-129. 00 μg/mL (r=0. 999 5), 5. 61-112. 20 μg/mL (r=0. 999 9), 4. 25-85. 00 μg/mL (r=0. 999 3), 9. 19-183. 80 μg/mL (r =0.999 8), and 11. 05-221. 00 μg/mL (r=0. 999 7), respectively; and their average recoveries and RSD were 98. 73% (1. 43%), 97. 63% (1. 28%), 99. 44% (1. 29%), 98. 33% (1. 38%), and 97. 36% (1. 37%), respectively. Conclusion The established joint wavelength switching HPLC gradient elution method is simple, accurate and reproducible; it can simultaneously determine the contents of darutoside, kirenol, darutigenol, fangchinoline and d-tetrandrine in Xixian Fengshi Wnn and can be used for quality control of Xixinn Fengshi Wan.